CN108603862A - The manufacturing method of simulated defect sample and its manufacturing method, the method for adjustment of ultrasonic examination determination condition, the inspection method of target raw material and sputtering target - Google Patents

The manufacturing method of simulated defect sample and its manufacturing method, the method for adjustment of ultrasonic examination determination condition, the inspection method of target raw material and sputtering target Download PDF

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CN108603862A
CN108603862A CN201880000346.8A CN201880000346A CN108603862A CN 108603862 A CN108603862 A CN 108603862A CN 201880000346 A CN201880000346 A CN 201880000346A CN 108603862 A CN108603862 A CN 108603862A
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flat
bottom hole
equivalent circle
raw material
circle diameter
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CN108603862B (en
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菅原裕明
西冈宏司
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Sumitomo Chemical Co Ltd
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Sumitomo Chemical Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/22—Details, e.g. general constructional or apparatus details
    • G01N29/30—Arrangements for calibrating or comparing, e.g. with standard objects
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/04—Analysing solids
    • G01N29/043—Analysing solids in the interior, e.g. by shear waves
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/04—Analysing solids
    • G01N29/06—Visualisation of the interior, e.g. acoustic microscopy
    • G01N29/0609—Display arrangements, e.g. colour displays
    • G01N29/0645—Display representation or displayed parameters, e.g. A-, B- or C-Scan
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/04—Analysing solids
    • G01N29/11—Analysing solids by measuring attenuation of acoustic waves
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/44—Processing the detected response signal, e.g. electronic circuits specially adapted therefor
    • G01N29/4409—Processing the detected response signal, e.g. electronic circuits specially adapted therefor by comparison
    • G01N29/4418—Processing the detected response signal, e.g. electronic circuits specially adapted therefor by comparison with a model, e.g. best-fit, regression analysis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/44—Processing the detected response signal, e.g. electronic circuits specially adapted therefor
    • G01N29/4409—Processing the detected response signal, e.g. electronic circuits specially adapted therefor by comparison
    • G01N29/4427—Processing the detected response signal, e.g. electronic circuits specially adapted therefor by comparison with stored values, e.g. threshold values
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/44—Processing the detected response signal, e.g. electronic circuits specially adapted therefor
    • G01N29/4409—Processing the detected response signal, e.g. electronic circuits specially adapted therefor by comparison
    • G01N29/4436—Processing the detected response signal, e.g. electronic circuits specially adapted therefor by comparison with a reference signal
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/02—Indexing codes associated with the analysed material
    • G01N2291/028—Material parameters
    • G01N2291/0289—Internal structure, e.g. defects, grain size, texture
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/04—Wave modes and trajectories
    • G01N2291/044—Internal reflections (echoes), e.g. on walls or defects
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/26—Scanned objects
    • G01N2291/263—Surfaces
    • G01N2291/2632—Surfaces flat
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

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Abstract

The simulated defect sample of the present invention is used to adjust the ultrasonic examination determination condition for the internal flaw for checking target raw material,Aforementioned analog defect sample has the substrate comprising the 1st face and 2nd face opposite with the 1st face,The counter sink with the 1st depth from aforementioned 1st surface side is formed on aforesaid base plate,And,A part in the bottom surface of aforementioned counter sink is formed with the flat-bottom hole with the 2nd depth from the bottom surface of aforementioned counter sink,When the equivalent circle diameter φ of aforementioned flat-bottom hole is less than 0.3mm,The equivalent circle diameter φ of aforementioned flat-bottom hole is 0.08 less than 0.40 relative to ratio φ/d of the 2nd depth d of aforementioned flat-bottom hole,The equivalent circle diameter φ of aforementioned flat-bottom hole be 0.3mm less than 0.4mm when,Aforementioned ratio φ/d is 0.1 less than 0.60,When the equivalent circle diameter φ of aforementioned flat-bottom hole is 0.4mm or more,Aforementioned ratio φ/d is 0.11 less than 1.60.

Description

The adjustment side of simulated defect sample and its manufacturing method, ultrasonic examination determination condition The manufacturing method of method, the inspection method of target raw material and sputtering target
Technical field
The present invention relates to the conditions that the ultrasonic examination for the internal flaw to checking target raw material measures to be adjusted Simulated defect sample and its manufacturing method, the method for adjustment of conditions of ultrasonic inspection, the inspection method of target raw material and splash The manufacturing method shot at the target.
Background technology
In the sputtering utilized extensively in semiconductor manufacturing field of flat panel etc., sputtering target has been used.To splashing Shoot at the target when being sputtered, if there is the defects of such as hole, oxide, foreign matter in the inside of target raw material, may occur because Paradoxical discharge caused by these defects.Due to the paradoxical discharge, the phenomenon that being referred to as " splash (splash) " is generated sometimes.Institute Splash is called, is a part of there is a phenomenon where melting, being attached to substrate and solidifying of target raw material, which may result in Wiring, short circuit between electrodes obtained by being formed a film by sputtering.
In order to inhibit the paradoxical discharge of target raw material, it is desirable that the inside of target raw material there is no fine defect (for example, φ 0.2mm or more).Therefore, it when manufacturing target raw material, needs to check that there is zero defect in the inside of target raw material.As the inspection Method has the method for the variation for the reflection echo that ultrasonic wave is observed using ultrasound inspection head.
Measurement accuracy when being checked using ultrasound inspection head to improve, what adjustment emitted from ultrasound inspection head The focus of ultrasonic wave.In order to which the focus to the ultrasonic wave emitted from ultrasound inspection head is adjusted, simulated defect sample is used. In simulated defect sample, it is provided with the hole with the size that the fine defect in target raw material is same degree.Moreover, make from The focus of the ultrasonic wave of ultrasound inspection head transmitting is directed at the hole, measures by the reflection echo of the bottom reflection in hole, and to ultrasound The sensitivity of wave inspection is adjusted.
Simulated defect sample has been recorded in patent document 1.The simulated defect sample has counter sink and is arranged on countersunk head The bottom surface in hole and the diameter flat-bottom hole smaller than the diameter of counter sink.Moreover, measuring by the reflection echo of the bottom reflection of counter sink With the reflection echo of the bottom reflection by flat-bottom hole, and the sensitivity of ultrasonic examination is adjusted.
For aforementioned previous simulated defect sample, due to being examined for the defect of large-scale industrial part, because And the diameter of flat-bottom hole is big.Therefore, the focus of the ultrasonic wave emitted from ultrasound inspection head is directly directed at small flat-bottom hole is Readily.
However, aforementioned previous simulated defect sample is not intended to check the simulated defect of the microscopic defect in target raw material Therefore sample to the simulated defect sample is directly applied to target raw material, then must reduce the diameter of flat-bottom hole.
Existing technical literature
Patent document
Patent document 1：JP2010-145401 bulletins
Invention content
Problems to be solved by the invention
The purpose of the present invention is to provide the items that the ultrasonic examination suitable for the inspection method to target raw material measures The manufacturing method of simulated defect sample and its manufacturing method, the inspection method of target raw material and sputtering target that part is adjusted.
The simulated defect sample of the present invention is for checking that the ultrasonic examination of the internal flaw of target raw material measures The simulated defect sample that condition is adjusted,
Aforementioned analog defect sample has the substrate comprising the 1st face and 2nd face opposite with the 1st face,
The counter sink with the 1st depth from aforementioned 1st surface side is formed on aforesaid base plate, also, in aforementioned countersunk head A part for the bottom surface in hole is formed with the flat-bottom hole with the 2nd depth from the bottom surface of aforementioned counter sink,
When the equivalent circle diameter φ of aforementioned flat-bottom hole is less than 0.3mm, the equivalent circle diameter φ of aforementioned flat-bottom hole is relative to preceding Ratio φ/the d for stating the 2nd depth d of flat-bottom hole is 0.08 less than 0.40,
The equivalent circle diameter φ of aforementioned flat-bottom hole be 0.3mm less than 0.4mm when, the equivalent circle of aforementioned flat-bottom hole is straight Diameter φ is 0.1 less than 0.60 relative to ratio φ/d of the 2nd depth d of aforementioned flat-bottom hole,
When the equivalent circle diameter φ of aforementioned flat-bottom hole is 0.4mm or more, the equivalent circle diameter φ of aforementioned flat-bottom hole relative to Ratio φ/d of 2nd depth d of aforementioned flat-bottom hole is 0.11 less than 1.60.
Herein, the equivalent circle diameter of so-called flat-bottom hole refers to diameter of a circle when flat-bottom hole is round；It is not in flat-bottom hole Refer to the diameter of a circle with the area of a circle of the area equation of flat-bottom hole when round.Specifically, the area of flat-bottom hole is remembered For S when, equivalent circle diameter φ be (4S/ π) 1/2.
Simulated defect sample according to the present invention is carrying out the condition that ultrasonic examination measures using simulated defect sample Adjustment in, adjust ultrasonic examination sensitivity when, even if by the focus pair of the ultrasonic wave emitted from ultrasound inspection head The bottom surface of quasi- counter sink can also identify the reflection echo from flat-bottom hole.
I.e., it is possible to which the focus alignment of the ultrasonic wave emitted from ultrasound inspection head to be easy to the bottom of the big counter sink of detection Face, and small flat-bottom hole is identified in this state.Therefore, ultrasound inspection head can be easily located at flat-bottom hole, make by from The operation of the bottom surface of the focus alignment flat-bottom hole of the ultrasonic wave of ultrasound inspection head transmitting becomes simple.
Therefore, simulated defect sample according to the present invention so that the sensitivity adjustment of ultrasonic examination is easy to carry out, and can contract The condition required time that the whole ultrasonic examination of minor measures.
In an embodiment of simulated defect sample, the equivalent circle diameter φ of aforementioned flat-bottom hole is 0.5mm or less.
It is difficult since the equivalent circle diameter φ of flat-bottom hole is 0.5mm hereinafter, therefore, flat-bottom hole is small according to aforementioned embodiments The focus of the ultrasonic wave emitted from ultrasound inspection head is directly directed at flat-bottom hole.In present embodiment, it can readily recognize Above-mentioned such flat-bottom hole for being difficult to Direct Recognition.
In an embodiment of simulated defect sample, the equivalent circle diameter φ of aforementioned flat-bottom hole be 0.1mm or more and Less than 0.3mm.
According to aforementioned embodiments, since the equivalent circle diameter φ of flat-bottom hole is 0.1mm less than 0.3mm, Flat-bottom hole is very small, but in the present embodiment, can readily recognize the flat-bottom hole.
In an embodiment of simulated defect sample, the condition that ultrasonic examination measures is for being 5MHz with frequency The condition that the ultrasonic examination that above ultrasonic wave is implemented measures.
In an embodiment of simulated defect sample,
Aforementioned counter sink and aforementioned flat-bottom hole have multigroup.
According to aforementioned embodiments, preferably aforementioned counter sink and aforementioned flat-bottom hole have multigroup.
The position of same depth is in simulated defect sample by being configured at the bottom surface of multigroup flat-bottom hole, so as to The focus of ultrasonic wave emit from ultrasound inspection head is adjusted, repeatedly the sensitivity adjustment of implementation ultrasonic examination, it therefore, can be into One step improves the precision of the sensitivity adjustment.In addition, the equivalent circle diameter φ of aforesaid plurality of flat-bottom hole identical can also that This is different.
In an embodiment of simulated defect sample, aforesaid base plate is by aluminium, copper, titanium, silver or includes these metals member The alloy of at least one of element is formed.
According to aforementioned embodiments, these materials for constituting substrate are easy in the manufacture (melting casting) of target raw material Generate the material of gap (defect).Therefore, it when manufacturing sputtering target using the target raw material formed by these materials, is used There is flawless ultrasonic examination inspection in investigation, therefore these materials are suitable for simulated defect sample.
The manufacturing method of simulated defect sample is the method for manufacturing following simulated defect samples, and the simulated defect sample is used It is adjusted in the condition that the ultrasonic examination of the internal flaw to checking target raw material measures, the manufacturing method has following Process：
It is formed on the substrate comprising the 1st face and 2nd face opposite with the 1st face deep with the 1st from aforementioned 1st surface side The process of the counter sink of degree；With
A part in the bottom surface of aforementioned counter sink forms the flat-bottom hole with the 2nd depth from aforementioned bottom surface, aforementioned flat The equivalent circle diameter φ of bottom outlet be less than 0.3mm when, make the equivalent circle diameter φ of aforementioned flat-bottom hole relative to aforementioned flat-bottom hole the 2nd Ratio φ/d of depth d is 0.08 less than 0.40, the equivalent circle diameter φ of aforementioned flat-bottom hole be 0.3mm less than When 0.4mm, make the equivalent circle diameter φ of aforementioned flat-bottom hole relative to ratio φ/d of the 2nd depth d of aforementioned flat-bottom hole be 0.1 with Above and less than 0.60, when the equivalent circle diameter φ of aforementioned flat-bottom hole is 0.4mm or more, make the equivalent circle diameter φ of aforementioned flat-bottom hole Ratio φ/d of the 2nd depth d relative to aforementioned flat-bottom hole be 0.11 less than 1.60 process.
When being used to adjust the condition of ultrasonic examination measurement by the simulated defect sample obtained by previous building methods so that The sensitivity adjustment of ultrasonic examination is easy to carry out, and can shorten the condition required time that adjustment ultrasonic examination measures.
In an embodiment of the manufacturing method of simulated defect sample, aforesaid base plate by aluminium, copper, titanium, silver or comprising The alloy of at least one of these metallic elements is formed.
According to aforementioned embodiments, these materials for constituting substrate are easy in the manufacture (melting casting) of target raw material Generate the material of gap (defect).Therefore, it when manufacturing sputtering target using the target raw material formed by these materials, is used There is flawless ultrasonic examination inspection in investigation.
The method for adjusting the condition that ultrasonic examination measures has following processes：
By ultrasound inspection head, from the 2nd of the substrate of aforementioned simulated defect sample towards the 1st surface launching ultrasonic wave, to preceding State the process that the reflection echo of counter sink is confirmed；
The reflection echo of counter sink based on aforementioned analog defect sample makes the focus of aforementioned ultrasonic be directed at aforementioned countersunk head The process of the bottom surface in hole；
It receives by the reflection echo of the bottom reflection of aforementioned counter sink, and receives by the flat of aforementioned analog defect sample The process of the reflection echo of the bottom reflection in hole；With
Based on the reflection echo from the bottom surface of aforementioned flat-bottom hole, the focus of aforementioned ultrasonic is made to be directed at aforementioned flat-bottom hole The process of bottom surface.
According to aforementioned method of adjustment, in the adjustment carried out to the condition that ultrasonic examination measures using simulated defect sample In, when adjusting the sensitivity of ultrasonic examination, even if the focus of the ultrasonic wave emitted from ultrasound inspection head is directed at countersunk head The bottom surface in hole can also be differentiated with the reflection echo of the bottom surface from counter sink, to bottom surface of the identification from flat-bottom hole Reflection echo.
I.e., it is possible to which the focus alignment of the ultrasonic wave emitted from ultrasound inspection head to be easy to the bottom of the big counter sink of detection Face, and small flat-bottom hole is identified in this state.Therefore, ultrasound inspection head can be easily located at flat-bottom hole, make by from The operation of the bottom surface of the focus alignment flat-bottom hole of the ultrasonic wave of ultrasound inspection head transmitting becomes simple.
Therefore, according to aforementioned method of adjustment so that the sensitivity adjustment of ultrasonic examination is easy to carry out, and it is super can to shorten adjustment The condition required time that sonic flaw detection measures.
In an embodiment of aforementioned method of adjustment, the condition that ultrasonic examination measures is for being 5MHz with frequency The condition that the ultrasonic examination that above ultrasonic wave is implemented measures.
The inspection method of target raw material has following processes：
Under conditions of the ultrasonic examination adjusted using aforementioned method of adjustment is measured, make ultrasonic examination on one side Head is scanned the process for emitting ultrasonic wave to target raw material on one side；
The process for measuring the reflection echo reflected by aforementioned target raw material；With
Based on through it is aforementioned measure obtain as a result, the process of the internal flaw to judge aforementioned target raw material.
According to aforementioned inspection method, by using the good ultrasonic examination assay method of precision, so as to sentence well The quality of targeting raw material.
In an embodiment of the manufacturing method of sputtering target, there are following processes：
Using aforementioned inspection method, come judge target raw material internal flaw process；With
Implement the process of mechanical processing to being judged as the internal target raw material essentially without defect.
In the other embodiment of the manufacturing method of sputtering target, there are following processes：
Using aforementioned inspection method, come judge aforementioned target raw material internal flaw process；With
By the aforementioned process for being judged as the internal target raw material essentially without defect and being engaged in supporting member.
According to the manufacturing method of aforementioned sputtering target, by using the good target raw material of quality, to which sputtering target can be improved Quality.
Invention effect
Simulated defect sample according to the present invention and its manufacturing method can easily set the item of ultrasonic examination measurement Part.
The method for the condition that adjustment ultrasonic examination through the invention measures, can be easy to carry out the spirit of ultrasonic examination Sensitivity adjusts.The inspection method of target raw material through the invention, can easily be determined that the quality of target raw material.Through the invention Sputtering target manufacturing method, the good sputtering target of quality can be manufactured.
Description of the drawings
[Fig. 1] to illustrate the invention in the definition graph of principle that measures of the ultrasonic examination that uses.
[Fig. 2] is the vertical view for the 1st embodiment for indicating the simulated defect sample of the present invention.
[Fig. 3] is the sectional view for the 1st embodiment for indicating the simulated defect sample of the present invention.
[Fig. 4] is the explanation illustrated to the method for using simulated defect sample to adjust the condition that ultrasonic examination measures Figure.
[Fig. 5] be indicate φ be 0.2mm, φ/d be 0.08 less than 0.40 when measurement signal oscillogram.
[Fig. 6] be indicate φ be 0.2mm, φ/d be 0.40 or more when measurement signal oscillogram.
[Fig. 7] is to indicate that φ is the oscillogram for measuring signal when 0.2mm, φ/d are less than 0.08.
[Fig. 8] is the stereogram of sputtering target.
[Fig. 9] is the sectional view for the 2nd embodiment for indicating the simulated defect sample of the present invention.
Specific implementation mode
Hereinafter, by embodiment illustrated, the present invention will be described in detail.
(the 1st embodiment)
Fig. 1 to illustrate the invention in the definition graph of principle that measures of the ultrasonic examination that uses.As shown in Figure 1, ultrasonic wave Flaw detection head 1 is used as a kind of ultrasonic examination inspection (UT in nondestructive inspection:Ultrasonic Testing).
Ultrasonic examination inspection is illustrated.The ultrasonic pulse generated by impulse sender is from ultrasound inspection head 1 It sends out, part of it is reflected on the surface of the internal flaw 2a of inspected body 2.Its back wave is received by ultrasound inspection head 1, It is converted into high frequency voltage.Inverted signal is shown in display via receiver, can confirm the position of defect 2a and big Small degree.In Fig. 1, defect 2a indicates hole.
Specifically, emitting ultrasonic wave U from ultrasound inspection head 1 on one side, make ultrasound inspection head 1 along inspected body on one side 2 surface 2b is moved to the right from the left side of Fig. 1.As is illustrated in the left side of fig. 1, when defect is not present in the inside of inspected body 2, If from ultrasound inspection head 1 emit ultrasonic wave U, from the surface 2b of inspected body 2 receive the 1st reflection echo E1, from be examined The back side 2c of body 2 receives the 2nd reflection echo E2.Measurement signal S1 at this time includes the 1st signal Z1 from the 1st reflection echo E1 With the 2nd signal Z2 from the 2nd reflection echo E2.
On the other hand, as shown in the right side of Fig. 1, in the inside existing defects 2a of inspected body 2, if from ultrasonic examination First 1 transmitting ultrasonic wave U, then receive the 1st reflection echo E1 from the surface 2b of inspected body 2, received from the back side 2c of inspected body 2 2nd reflection echo E2 receives the 3rd reflection echo E3 from the surface of the defect 2a of inspected body 2.Measurement signal S2 at this time includes The 1st signal Z1, the 2nd signal Z2 from the 2nd reflection echo E2 from the 1st reflection echo E1 and come from the 3rd reflection echo E3 The 3rd signal Z3.As described above, can confirm defect 2a by the 3rd signal Z3.
In the present invention, ultrasound inspection head 1 is examined for the internal flaw of target raw material.Target raw material be used to sputter Target.
Fig. 2 is the vertical view for the 1st embodiment for indicating the simulated defect sample of the present invention.Fig. 3 is to indicate the present invention's The sectional view of 1st embodiment of simulated defect sample.As shown in Figures 2 and 3, simulated defect sample 10 has substrate 10.Base Plate 10 includes the 1st face 11a and 2nd face 11b opposite with the 1st face 11a.
The counter sink 12 with the 1st depth d1 from the 1st face sides 11a is formed on the substrate 10, also, in counter sink 12 A part of bottom surface 12a forms the flat-bottom hole 13 with the 2nd depth d2 from the bottom surface 12a of counter sink 12.1st depth d1 and The relationship of 2 depth d2 is not particularly limited, when the thickness of simulated defect sample 10 becomes larger, especially the 2nd depth d2 be more than 4mm When, preferably the 1st depth d1 is more than the 2nd depth d2.Counter sink 12 and flat-bottom hole 13 are circle, and flat-bottom hole 13 is arranged at counter sink A part of 12 bottom surface 12a, but it is preferred that being configured in same heart shaped when from the 2nd face sides 11b, that is, flat-bottom hole 13 It is configured in the center of counter sink 12.By making flat-bottom hole 13 be configured in same heart shaped with counter sink 12, thus especially flat-bottom hole Diameter hour, it will be easy find flat-bottom hole position.The diameter phi 1 of counter sink 12 is more than the diameter phi 2 of flat-bottom hole 13.Separately Outside, for the bottom surface of counter sink, flat-bottom hole, in order to make it be easy the ultrasonic wave that reflection emits from ultrasound inspection head, lead to It is often general plane, preferably plane, the preferably plane relative to the direction of illumination of ultrasonic wave substantially vertical (preferred vertical).
For flat-bottom hole 13 equivalent circle diameter φ for ratio φ/d of the 2nd depth d of flat-bottom hole 13, it is flat When the equivalent circle diameter φ in hole 13 is less than 0.3mm, φ/d is 0.08 less than 0.40, the equivalent circle diameter φ of flat-bottom hole 13 When for 0.3mm less than 0.4mm, φ/d is 0.1 less than 0.60, and the equivalent circle diameter φ of flat-bottom hole 13 is When 0.4mm or more, φ/d is 0.11 less than 1.60.In this embodiment, the 2nd depth d of flat-bottom hole 13 refer to from The 2nd depth d2 of the bottom surface 12a of counter sink 12 to the bottom surface 13a of flat-bottom hole 13.As the size according to equivalent circle diameter φ The reasons why making ratio φ/d relative to depth d change, be because：When ratio φ/d is big (the bottom surface 12a of counter sink 12 with it is flat The distance hour of the bottom surface 13a in hole 13), the reflection echo of the bottom surface 12a of counter sink 12 is too strong, therefore, the bottom with flat-bottom hole 13 The reflection echo of face 13a is overlapped, and leads to not open with the echo free of the bottom surface 13a of flat-bottom hole 13.In addition, ratio φ/d hours (when the bottom surface 12a of counter sink 12 is big at a distance from the bottom surface 13a of flat-bottom hole 13), especially φ hours, the bottom surface of flat-bottom hole 13 The reflection echo of 13a itself dies down, therefore becomes difficult to detect.
Since flat-bottom hole 13 is circle, the equivalent circle diameter φ of flat-bottom hole 13 refers to diameter of a circle φ 2.It needs to illustrate , flat-bottom hole and it is non-circular when, refer to the diameter of a circle with the area of a circle of the area equation of flat-bottom hole.Specifically, When the area of flat-bottom hole is denoted as S, equivalent circle diameter φ is (4S/ π)1/2。
According to aforementioned analog defect sample 10, the condition that ultrasonic examination measures is being carried out using simulated defect sample 10 Adjustment in, adjust ultrasonic examination sensitivity when, even if by the focus pair of the ultrasonic wave emitted from ultrasound inspection head The bottom surface 12a of quasi- counter sink 12 can also identify the reflection echo of the bottom surface 13a from flat-bottom hole 13.
Specifically, as shown in figure 4, by ultrasound inspection head 1, surpass from the 2nd face 11b of substrate 11 to the 1st face 11a transmittings Sound wave U.At this point, the focus of the ultrasonic wave emitted from ultrasound inspection head to be aligned to the bottom surface 12a of counter sink 12.Then, from base 2nd face 11b of plate 11 receives the 1st reflection echo E11, and the 2nd reflection echo E31 is received from the bottom surface 12a of counter sink 12, from flat The bottom surface 13a in hole 13 receives the 3rd reflection echo E32.
As shown in figure 5, the signal S11 of measuring at this time includes the 1st signal Z11 from the 1st reflection echo E11, comes from the 2nd The 2nd signal Z31 of reflection echo E31 and the 3rd signal Z32 from the 3rd reflection echo E32.In Fig. 5, horizontal axis indicates between measuring Away from the longitudinal axis indicates the intensity (gain) of reflection echo.As described above, can identify the 3rd signal Z32 from signal S11 is measured, therefore, It can identify the position of the bottom surface 13a of flat-bottom hole 13.Show that the diameter phi 2 (equivalent circle diameter φ) of flat-bottom hole 13 is in Fig. 5 The case where 0.2mm.
Therefore, because the equivalent circle diameter φ of flat-bottom hole 13 be less than 0.3mm, ratio φ/d be 0.08 less than 0.40, thus the focus of the ultrasonic wave emitted from ultrasound inspection head can be aligned to the bottom for the big counter sink 12 for being easy detection Face 12a, and small flat-bottom hole 13 is identified in this state.As a result, then, ultrasound inspection head 1 can be easily located at flat Bottom outlet 13 makes the operation by the bottom surface 13a that the focus of the ultrasonic wave emitted from ultrasound inspection head is directed at flat-bottom hole 13 become letter It is single.Therefore, the sensitivity adjustment of ultrasonic examination is easy to carry out, and it is required can to shorten the condition that adjustment ultrasonic examination measures Time.
In contrast, when ratio φ/d is 0.40 or more, as shown in fig. 6, measurement signal S12 at this time includes to come from the 1st The 1st signal Z11 of reflection echo E11 (the 2nd face 11b of substrate 11) and come from the 2nd (bottom surfaces of counter sink 12 reflection echo E31 The 2nd signal Z31 12a).The 3rd signal Z32 and the 2nd signal from the 3rd reflection echo E32 (the bottom surface 13a of flat-bottom hole 13) Z31 is overlapped, None- identified.If in short, not increasing the bottom surface 13a's from the bottom surface 12a of counter sink 12 to flat-bottom hole 13 fully Distance (if d becomes smaller) causes since the 2nd reflection echo E31 from counter sink 12 is very strong from flat-bottom hole 13 3rd reflection echo E32 is Chong Die with from the 2nd reflection echo E31 of counter sink 12, can not separate the 3rd from flat-bottom hole 13 Reflection echo E32.None- identified flat-bottom hole 13 as a result,.
On the other hand, when ratio φ/d is less than 0.08, as shown in fig. 7, measurement signal S13 at this time includes anti-from the 1st It is emitted back towards the 1st signal Z11 of wave E11 (the 2nd face 11b of substrate 11) and comes from the 2nd (bottom surfaces of counter sink 12 reflection echo E31 The 2nd signal Z31 12a).The 3rd signal Z32 from the 3rd reflection echo E32 (the bottom surface 13a of flat-bottom hole 13) is small, Wu Fashi Not.If in short, excessive (if d becomes larger) to the distance of the bottom surface 13a of flat-bottom hole 13 from the bottom surface 12a of counter sink 12, from flat The focus of 3rd reflection echo E32 of bottom outlet 13 deviates, and the 3rd reflection echo E32 from flat-bottom hole 13 dies down, and detects flat-bottom hole 13 become difficult.When the equivalent circle diameter φ of aforementioned flat-bottom hole is less than 0.3mm, φ/d is preferably 0.08 less than 0.40, More preferably 0.08 or more 0.3 hereinafter, further preferably 0.08 or more 0.27 or less.In addition, the equivalent circle of usual flat-bottom hole Diameter phi is 0.1mm or more.
The equivalent circle diameter φ of flat-bottom hole 13 be 0.3mm less than 0.4mm when, ratio φ/d is 0.1 or more and small Therefore, same as Fig. 5 in 0.60, the sensitivity adjustment of ultrasonic examination is easy to carry out, and can shorten adjustment ultrasonic examination and measure The condition required time.In contrast, when ratio φ/d is 0.60 or more, None- identified flat-bottom hole 13 same as Fig. 6. On the other hand, when the equivalent circle diameter φ of flat-bottom hole 13 is less than 0.3mm, None- identified flat-bottom hole 13 same as Fig. 7.It is aforementioned flat The equivalent circle diameter φ of bottom outlet be 0.3mm less than 0.4mm when, φ/d is preferably 0.1 less than 0.60, more preferably For 0.1 or more 0.5 hereinafter, further preferably 0.1 or more 0.4 or less.
When the equivalent circle diameter φ of flat-bottom hole 13 is 0.4mm or more, ratio φ/d is 0.11 less than 1.60, because This, same as Fig. 5, the sensitivity adjustment of ultrasonic examination is easy to carry out, and can shorten the condition institute that adjustment ultrasonic examination measures The time needed.In contrast, when ratio φ/d is 1.60 or more, None- identified flat-bottom hole 13 same as Fig. 6.On the other hand, When the equivalent circle diameter φ of flat-bottom hole 13 is less than 0.11mm, None- identified flat-bottom hole 13 same as Fig. 7.The equivalent of flat-bottom hole 13 Circular diameter φ be 0.4mm or more when, φ/d be preferably 0.11 less than 1.60, more preferably 0.11 or more 1.1 hereinafter, into One step is preferably 0.11 or more 0.9 or less.
According to aforementioned analog defect sample 10, the equivalent circle diameter φ of flat-bottom hole 13 is preferably 0.5mm or less.At this point, flat Bottom outlet 13 is small, and the bottom surface 13a that the focus of the ultrasonic wave emitted from ultrasound inspection head is directly aligned to flat-bottom hole 13 is difficult. However, since ratio φ/d is in the range of above-mentioned the application embodiment, therefore, it is possible to by will be from ultrasound inspection head The focus of the ultrasonic wave of transmitting is directed at the bottom surface 12a of counter sink 12 to identify flat-bottom hole 13.Therefore, it can readily recognize and be difficult to directly Connect the flat-bottom hole 13 of identification.
The equivalent circle diameter φ of flat-bottom hole 13 is preferably 0.1mm less than 0.3mm, more preferably 0.1mm or more 0.25mm or less.At this point, flat-bottom hole 13 is very small, but in the present embodiment, the flat-bottom hole 13 can be readily recognized.
The material of substrate 11 is not particularly limited, as long as by the ceramics such as metal, alloy, oxide, nitride or sintering The material that body is constituted, can be made of the material of electric conductivity, suitable material is selected according to purposes, purpose.As Such material can enumerate such as aluminium, copper, titanium, silver or alloy, tin dope oxygen comprising at least one of these metallic elements Change indium (ITO), aluminium-doped zinc oxide (AZO), Ga-doped zinc oxide (GZO), titanium doped zinc oxide, In-Ga-Zn systems combined oxidation Object (IGZO).Wherein, aluminium, copper, titanium, silver or the alloy comprising at least one of these metallic elements are cast by melting To manufacture the material for easy ting produce gap (defect) when target raw material.Therefore, the target raw material formed by these materials are being utilized Come when manufacturing sputtering target, it is preferable to use the simulated defect sample 10 formed by these materials carries out ultrasonic examination inspection.In addition, Can substrate 11 be constituted by metal material identical with target raw material, can be appropriately setting for checking that the ultrasonic wave of target raw material is visited Hinder the condition measured.
Next, with reference to Fig. 3, the manufacturing method of aforementioned analog defect sample 10 is illustrated.
The counter sink 12 with the 1st depth d1 from the 1st face sides 11a is formed on the substrate 11.Then, in counter sink 12 A part of bottom surface 12a forms the flat-bottom hole 13 with the 2nd depth d2 from the 12a of bottom surface.At this point, the equivalent circle of flat-bottom hole 13 is straight When diameter φ is less than 0.3mm, make the equivalent circle diameter φ (being diameter phi 2 in the embodiment) of flat-bottom hole 13 relative to flat-bottom hole Ratio φ/d of 13 the 2nd depth d (being the 2nd depth d2 in the embodiment) is 0.08 less than 0.40, flat-bottom hole 13 Equivalent circle diameter φ be 0.3mm less than 0.4mm when, make flat-bottom hole 13 equivalent circle diameter φ (in the embodiment, For diameter phi 2) relative to the 2nd depth d (being the 2nd depth d2 in the embodiment) of flat-bottom hole 13 ratio φ/d be 0.1 with Above and less than 0.60, when the equivalent circle diameter φ of flat-bottom hole 13 is 0.4mm or more, make the equivalent circle diameter φ of flat-bottom hole 13 (should Be diameter phi 2 in embodiment) relative to flat-bottom hole 13 the 2nd depth d (in the embodiment, be the 2nd depth d2) ratio φ/d is 0.11 less than 1.60.
By the way that simulated defect sample 10 to be used to adjust the condition of ultrasonic examination measurement, so that ultrasonic examination Sensitivity adjustment is easy to carry out, and can shorten the condition required time that adjustment ultrasonic examination measures.In addition, in setting institute's phase When the flat-bottom hole 13 of the depth of prestige, for the common maximum length of drill bit, diameter more hour is shorter, is 2~10mm left The right side, therefore, the length of drill bit decide the speed of the adjustment.However, in present embodiment, the processing for carrying out counter sink 12 is straight Near to required depth, thus flat-bottom hole 13 can be opened up in desired position.
Next, with reference to Fig. 4, the method to using aforementioned analog defect sample 10 to adjust the condition that ultrasonic examination measures It illustrates.
By ultrasound inspection head 1, emits ultrasonic wave U from the 2nd face 11b of substrate 11 to the 1st face 11a, will be visited from ultrasonic wave Hinder the bottom surface 12a of the focus alignment counter sink 12 for the ultrasonic wave that hair is penetrated.
Then, the 2nd reflection echo E31 reflected by the bottom surface 12a of counter sink 12 is received, and is received by flat-bottom hole 13 3rd reflection echo E32 of bottom surface 13a reflections.Then, it is based on the 3rd reflection echo E32, it is super by what is emitted from ultrasound inspection head The bottom surface 13a of the focus alignment flat-bottom hole 13 of sound wave, adjusts the focus of the ultrasonic wave.
Even if if the focus of the ultrasonic wave emitted from ultrasound inspection head is directed at counter sink 12 can with from counter sink 12 The 2nd reflection echo E31 of bottom surface 12a differentiate, to the 3rd reflection echo of bottom surface 13a of the identification from flat-bottom hole 13 E32.As set forth above, it is possible to which the focus alignment of the ultrasonic wave emitted from ultrasound inspection head to be easy to the big counter sink 12 of detection Bottom surface 12a, and identify small flat-bottom hole 13 in this state.Therefore, when setting the condition that ultrasonic examination measures, can hold It changes places and ultrasound inspection head 1 is positioned at flat-bottom hole 13, so that the focus for the ultrasonic wave that will emit from ultrasound inspection head is aligned flat The operation of the bottom surface 13a of bottom outlet 13 becomes simple.Therefore, the sensitivity adjustment of ultrasonic examination is easy to carry out, and can shorten adjustment The condition required time that ultrasonic examination measures.
Next, referring to Fig.1, being illustrated to the inspection method of target raw material.
Under conditions of the ultrasonic examination adjusted using aforementioned method of adjustment is measured, make ultrasonic examination on one side First 1 is scanned, on one side to target raw material (inspected body 2) transmitting ultrasonic wave U.Then, measurement is reflected anti-by target raw material It is emitted back towards wave.Then, based on measuring as a result, judging whether target raw material are non-defective unit.Therefore, by using the good ultrasound of precision Wave inspection head 1 can judge the quality of target raw material well.
Next, the manufacturing method to sputtering target illustrates.
One embodiment of above-mentioned manufacturing method has following processes：Judge target raw material using aforementioned inspection method Internal flaw, to inside essentially without defect target raw material implement mechanical processing.
As mechanical processing, cutting processing, milling cutter processing, lathe process, slotting cutter processing etc. can be enumerated.By implementing machine Tool is processed, and can be manufactured by being finish-machined to desired size, surface state.
In the other embodiment of above-mentioned manufacturing method, judge that the inside of target raw material lacks using aforementioned inspection method It falls into.Then, as shown in figure 8, will be judged as the internal target raw material 6 essentially without defect is engaged in supporting member 7.This Place, refer to essentially without defect, using aforementioned inspection method check target raw material when, can't detect defect, alternatively, not with Flat-bottom hole is identical size or larger sized defect.Hereinafter, the target raw material by inside essentially without defect are known as sometimes " non-defective unit ".
Target raw material 6 can be processed to generally plate like, and the method for being processed into plate is not particularly limited.For example, will pass through Melt, cuboid, cylindric target obtained from casting the plastic processings such as process for rolling processing, extrusion process, forging, Then implement the mechanical processings such as cutting processing, milling cutter processing, lathe process, slotting cutter processing, it as a result, can be by being finish-machined to Desired size, surface state manufacture.
As the composition of target raw material, as long as in the film forming based on sputtering method it is usually workable by metal, alloy, The material that the ceramics such as oxide, nitride or sintered body are constituted, is not particularly limited, is suitably selected according to purposes, purpose Select target.As aforementioned target raw material, aluminium, copper, titanium, silver or using them as the alloy of principal component, tin dope oxygen can be enumerated Change indium (ITO), aluminium-doped zinc oxide (AZO), Ga-doped zinc oxide (GZO), titanium doped zinc oxide, In-Ga-Zn systems combined oxidation Object (IGZO) etc..In order to play the effect of the present invention, preferably aluminium, copper, titanium, silver or using them as the alloy of principal component, more preferably The aluminium of high-purity.
Shape, the size of target raw material 6 are not particularly limited, the plate of disk-shaped or long size can be formed as. When target raw material 6 are disk-shaped, diameter is, for example, 100mm~700mm, preferably 250mm~500mm, and more preferably 300mm~ 450mm.When target raw material 6 are the plate of long size, the length of short side direction is, for example, 100mm~2000mm, preferably 150mm ~1500mm, more preferably 180mm~1000mm.In addition, the length of long side direction is, for example, 100mm~4000mm, preferably 1000mm~3500mm, more preferably 2200mm~3000mm.It should be noted that the length and short side direction of long side direction Length may be the same or different.
Supporting member 7 is such as aluminium, copper by fine copper, Cu-Cr alloys, A2024 alloys, A5052 alloys or based on them The alloy of ingredient is formed.As supporting member, it is plectane that can mainly use backer board (backing plate), target raw material 6 When shape, backer board can be formed to have the diameter circle bigger or same or more smaller than its than the upper surface of target raw material 6 Shape upper surface it is disk-shaped.When target raw material 6 are the plate of long size, backer board can be formed to have by than target raw material 6 The plate of the long size for the upper surface that long or same or slightly shorter than it length short side and long side is constituted.In addition, target is former When material 6 is disk-shaped, the mainly supporting member by being constituted for configuring the ring portion of target raw material 6 can be used.Aforementioned bearing structure Part, which preferably has, can be used for the fixed flange part of sputter equipment.
The welding such as engagement for example, electron beam welding, diffusion engagement, solder.Sputtering target 5 can be manufactured as a result,.It can be right Target raw material after ultrasonic examination inspection are engaged in the target raw material after supporting member and implement mechanical processing, are finish-machined to institute Desired size, surface state., it is preferable to use milling machine, NC milling machines, machining center (machining for mechanical processing Center), lathe, NC lathes etc..
Therefore, by using the good target raw material 6 of quality, the quality of sputtering target 5 can be improved.
(the 2nd embodiment)
Fig. 9 is the sectional view for the 2nd embodiment for indicating the simulated defect sample of the present invention.2nd embodiment is real with the 1st The quantity of the counter sink and flat-bottom hole of applying mode is different.The different structures are illustrated below.It should be noted that In 2nd embodiment, reference numeral identical with the 1st embodiment is structure identical with the 1st embodiment, therefore omits it Explanation.
As shown in figure 9, in simulated defect sample 10A, counter sink 121,122,123 and flat-bottom hole 131,132,133 are deposited Multigroup (being 3 groups in the embodiment).The equivalent circle of the flat-bottom hole 131,132,133 of multigroup (being 3 groups in the embodiment) Diameter phi is different from each other.
Specifically, the 1st counter sink 121 and the 1st flat-bottom hole 131, the 2nd counter sink 122 and the 2nd flat-bottom hole 132 and the 3rd Counter sink 123 and the 3rd flat-bottom hole 133 configure in one direction along the 1st face 11a of substrate 11.
The diameter phi 21 (equivalent circle diameter φ) of 1st flat-bottom hole 131, the 22 (equivalent circle of diameter phi with the 2nd flat-bottom hole 132 Diameter phi), it is different from each other with the diameter phi 23 (equivalent circle diameter φ) of the 3rd flat-bottom hole 133.Each diameter phi 21, φ 22, φ 23 are excellent It is selected as 0.5mm or less.For example, diameter phi 21 is 0.2mm, diameter phi 22 is 0.3mm, and diameter phi 23 is 0.4mm.
In present embodiment, the diameter phi 11 of the 1st counter sink 121 is sunk with the diameter phi 12 of the 2nd counter sink 122, with the 3rd The diameter phi 13 of head bore 123 is identical in fig.9, but can also be different.1st depth d11 of the 1st counter sink 121 and the 2nd countersunk head It is the 1st depth d12 in hole 122, identical in fig.9 as the 1st depth d13 of the 3rd counter sink 123, but can also be different.1st is flat The 2nd depth d21 in hole 131, the 2nd depth d23 with the 2nd depth d22 of the 2nd flat-bottom hole 132, with the 3rd flat-bottom hole 133 are in Fig. 9 In it is identical, but can also be different.
The equivalent circle diameter φ (diameter phi 21) of 1st flat-bottom hole 131 is less than 0.3mm, and the equivalent circle of the 1st flat-bottom hole 131 is straight Diameter φ is 0.08 less than 0.40 relative to ratio φ/d of the 2nd depth d (the 2nd depth d21) of the 1st flat-bottom hole 131.
The equivalent circle diameter φ (diameter phi 22) of 2nd flat-bottom hole 132 is 0.3mm less than 0.4mm, the 2nd flat-bottom hole Ratio φ/ds of the 132 equivalent circle diameter φ (diameter phi 22) relative to the 2nd depth d (the 2nd depth d22) of the 2nd flat-bottom hole 132 For 0.1 less than 0.60.
The equivalent circle diameter φ (diameter phi 23) of 3rd flat-bottom hole 133 is 0.4mm or more, the equivalent circle of the 3rd flat-bottom hole 133 Diameter phi (diameter phi 23) is 0.11 or more relative to ratio φ/d of the 2nd depth d (the 2nd depth d23) of the 3rd flat-bottom hole 133 And it is less than 1.60.
According to aforementioned analog defect sample 10A, other than the effect of aforementioned 1st embodiment, due to equivalent circle diameter The flat-bottom hole of φ is very small, thus considers machining accuracy, and setting is multigroup, with positioned at the 2nd face away from simulated defect sample 10A The mode of the position of the identical distances of 11b configures multigroup flat-bottom hole.Therefore, super by emitting from ultrasound inspection head in adjusting The focus of sound wave and while adjusting the sensitivity of ultrasonic examination, carry out identical scan operation, so as to improve ultrasonic examination Sensitivity adjustment.It should be noted that for the group number of counter sink and flat-bottom hole, although illustrating 3 groups of feelings in fig.9 Condition, but may be 2 groups or 4 groups or more.In addition, multigroup flat-bottom hole can be respectively different diameter, it can also all phases Same diameter.
When the diameter of multigroup flat-bottom hole is respectively different, it can be directed to various sizes of defect, carry out the sensitive of higher precision Degree adjustment.
Hereinafter, the above embodiment is described in detail.
(about ultrasonic examination assay method)
Ultrasonic examination assay method includes A sweep, B-scan, C-scan this 3 kinds of assay methods.For example, being described in super Sound wave visits Check mapping device AT シ リ ー ズ (Ji Foundation Knitting) M671-HB-1 (ultrasonic investigation mapping device AT series (compiling on basis) M671-HB-1)(Hitachi Kenki FineTech Co.,Ltd.)。
So-called A sweep indicates the Temporal changes of the reflection echo at certain point, can be by being applied with monitorings such as oscilloscope tubes It is obtained to the voltage of ultrasonic sensor.In this method, according to whether there is or not reflection echos, to estimate the presence of foreign matter, defect etc., In addition, by measuring distance, its depth can be calculated.
A sweep is the information of certain point, and in contrast, so-called B-scan will be along the time of the reflection echo of certain straight line Property variation planar development, indicated as the plane information of depth direction.
So-called C-scan indicates the plane information of the reflection echo at the certain depth of measuring samples, can be by waiting for sample Ultrasound inspection head is set to be scanned to obtain along in-plane on product.This method can at one stroke will be in measuring samples whole region Internal state visualization.When being detected to the fine defect distribution in target surface whole region, flaw size, it is applicable in C Scanning method.
In the assay method of the present embodiment, the assay method of C-scan is utilized.It should be noted that the survey as the present invention Determine method, can also be used A sweep, B-scan assay method.
(focusing method when about the condition for adjusting ultrasonic examination measurement)
Simulated defect sample is put into screw clamp, it is made to be impregnated in water, ultrasound inspection head, which is configured at simulation, to be lacked Fall into the position of 10~500mm of surface, preferably 50~200mm, more preferable 75~150mm of sample or so.At this point, it is preferred that ultrasound Wave inspection head also is located in water.C-scan is carried out for the 2nd face whole face of simulated defect sample, counter sink is confirmed.It will surpass Sonic flaw detection head is moved to the counter sink confirmed, by ultrasound inspection head be configured at the surface 0.1 of simulated defect sample~ The position of 200mm, preferably 1~100mm, more preferable 3~50mm or so confirm the reflection echo height of counter sink.Into Row operates and ultrasound inspection head is made to be moved along the upper and lower directions of simulated defect sample.At this point, it is maximum to find out reflection echo height Position.The maximum position of reflection echo height is alignment position of the focus in counter sink.
(about simulated defect sample)
When carrying out C-scan to simulated defect sample, carry out with needing the entire surface for spreading the 2nd face of simulated defect sample Scanning.Therefore, the 1st face (face for offering counter sink of simulated defect sample) of simulated defect sample and the 2nd face (simulated defect The shadow surface of the ultrasonic wave of sample) there must be substantially vertical, preferred vertical the plane relative to the direction of illumination of ultrasonic wave.Mould The 1st face and the 2nd face of quasi- defect sample need general planar, preferably flat, and surface roughness is preferably 1.0 μm or less.
Multiple counter sinks can be opened up on simulated defect sample, it is same depth or different depths that can make multiple counter sinks Degree.It can want to implement to surpass to freely select by opening up the flat-bottom hole consistent with flaw size to be confirmed from counter sink The flaw size of sonic flaw detection can freely select the depth for wanting to carry out ultrasonic examination according to the depth location of flat-bottom hole Direction.
When carrying out ultrasonic examination in the thickness direction whole face of target raw material, it is preferred that the thickness of simulated defect sample Degree is identical as the thickness of target raw material, and the position of flat-bottom hole is configured in the center of thickness direction.The thickness of simulated defect sample When identical as the thickness of target raw material, the determination condition adjusted using simulated defect sample can not be modified, and The flaw detection of the internal flaw of target is carried out immediately.
It, can be in the central portion tune of thickness direction when the position of the flat-bottom hole of target raw material is configured in the center of thickness direction Whole sensitivity, thus be scanned suitable for the thickness direction whole region throughout target raw material.
The thickness of simulated defect sample can be different from the thickness of target raw material, as long as the shadow surface irradiated from ultrasonic wave The distance of (the 2nd face) to flat-bottom hole is identical at a distance from the surface to central portion from target raw material.
(about measurement in water)
When adjusting conditions of ultrasonic inspection using simulated defect sample, using water as medium.Ultrasonic medium includes Vibration is easy tod produce to carry out the medium of conduct acoustic waves and be difficult to the medium of conduct acoustic waves.Indicate the physics of the difficulty of above-mentioned propagation Amount is referred to as natural acoustic impedance (Z), and density is denoted as ρ, is indicated by Z=ρ c.C is the velocity of sound, is the distinctive value of substance.In order to be easy Ultrasonic wave is propagated, usually usable water is as medium.Water is not particularly limited, as long as the impurity not comprising a large amount of particle shape, Dust etc. can enumerate the use of such as tap water, pure water.
As medium, in addition to water, oily (Water-soluble cutting oil agent, water insoluble cutting oil agent, half-dried use also can be used Machining fluid, motor oil (motor oil), machinery oil (machine oil) etc.), organic solvent (methanol, ethyl alcohol, propyl alcohol, third Ketone, ethylene glycol etc.) etc. liquid or glycerine, vaseline isogel material.Preferably, it is contemplated that the difficulty of the difficulty or ease, processing started with Easily, wash difficulty or ease, the difficulty or ease of maintenance, discarded difficulty or ease, in price, it is preferable to use water.
It is preferred that implementing the adjustment for using simulated defect sample to carry out, the inspection of target raw material in water.
(frequency about ultrasound inspection head when measuring)
Usually it is measured with the frequency of the ultrasound inspection head of 5MHz or more, it is excellent when the diameter of flat-bottom hole is less than 0.5mm Choosing makes the frequency of ultrasound inspection head be measured for 10MHz or more, and more preferably 10MHz or more 50MHz are hereinafter, further Preferably 12MHz or more 30MHz are hereinafter, particularly preferably 13MHz or more 20MHz or less.
When ultrasonic frequency becomes larger, the wavelength of ultrasonic wave shortens, and therefore, resolution ratio when ultrasonic examination improves.Target is former Material is aluminium (density 2.7g/cm3) when, need high-frequency ultrasonic wave.When target raw material are aluminium, if the diameter of flat-bottom hole is small In 0.5mm, then optimized frequency is 10MHz or more.If the diameter of flat-bottom hole is less than 0.3mm, optimized frequency is 12MHz or more.
(about counter sink)
The diameter of counter sink has to be larger than the diameter of flat-bottom hole.Due to opening up flat-bottom hole after opening up counter sink, so needing It is the size for the degree for making drill bit enter, therefore, the diameter of counter sink is preferably 5mm or more.In same simulated defect sample It is upper that if counter sink is excessive, the hole count that can be opened up in simulated defect sample surface is reduced when making multiple counter sinks, alternatively, Simulated defect sample itself becomes too much, and therefore, the diameter of counter sink is preferably 20mm or less.
(the measurement spacing about ultrasound inspection head)
In order to measure fine defect, the measurement spacing of ultrasonic wave is the smaller the better, if but measure spacing it is too small, measure Time consumption is excessive.Therefore, it is preferably 0.05mm or more and 1.0mm or less to measure spacing.So-called measurement spacing, is to instigate ultrasound Measuring interval when wave inspection head is scanned along in-plane.
It should be noted that the present invention is not limited to above-mentioned embodiment, it can be in the range of the purport without departing from the present invention Inside it is designed change.For example, can various combinations be carried out for the 1st embodiment and the respective characteristic point of the 2nd embodiment.
(embodiment)
Investigate the relationship between the equivalent circle diameter φ of flat-bottom hole, the 2nd depth d and the detection of flat-bottom hole of flat-bottom hole.Make For simulated defect sample, it is circle to make the shape of flat-bottom hole, and it is 0.2mm, 0.3mm, 0.4mm to make equivalent circle diameter (diameter) φ. It is Al-0.5%Cu to make the raw material of simulated defect sample.The surface roughness of the ultrasonic irradiation side of simulated defect sample is set to be 0.07μm.As measurement device, use " FSLINE " of Hitachi Power Solutions.
First, in preparation before the assay, by ultrasound inspection head " I3-1506S-50mm " (frequency 15MHz, focal length For 50mm) it is installed on measurement device.
Then, by be provided with counter sink it is face-down in a manner of, simulated defect sample is positioned over to the sink of measurement device It is interior.Tap water has been prefilled in sink.Then, ultrasonic wave is irradiated by ultrasound inspection head, confirms the reflection from counter sink The focus of ultrasonic wave, is directed at the bottom surface of counter sink by echo, and then confirmed the reflection echo from flat-bottom hole in this state. At this point, gain is set as 22dB.The detection data of flat-bottom hole when showing for focus to be directed at the bottom surface of counter sink in table 1.Table 1 In, it will detect that flat-bottom hole is expressed as "○" as the case where defect, will fail to detect flat-bottom hole as table the case where defect It is shown as "×".In table 1, the region of "○" is shown with shade.
[table 1]
As shown in Table 1, when equivalent circle diameter φ is 0.2mm, if the 2nd depth d be 0.75mm or more and 2.50mm hereinafter, if It can detect flat-bottom hole.On the other hand, it if the 2nd depth d is 0.50mm or less or 3.00mm or more, is difficult to detect flat Hole.
In addition, when equivalent circle diameter φ is 0.25mm, if the 2nd depth d be 0.75mm or more and 3.00mm hereinafter, if can examine Measure flat-bottom hole.On the other hand, it if the 2nd depth d is 0.50mm or less or 3.50mm or more, is difficult to detect flat-bottom hole.
When equivalent circle diameter φ is 0.3mm, if the 2nd depth d be 0.75mm or more and 3.00mm hereinafter, if can detect it is flat Bottom outlet.On the other hand, it if the 2nd depth d is 0.50mm or less or 3.50mm or more, is difficult to detect flat-bottom hole.
When equivalent circle diameter φ is 0.4mm, if the 2nd depth d be 0.50mm or more and 3.50mm hereinafter, if can detect it is flat Bottom outlet.On the other hand, it if the 2nd depth d is 0.25mm or less or 4.00mm or more, is difficult to detect flat-bottom hole.
Relationship between equivalent circle diameter φ, the 2nd depth d and φ/d is shown in table 2.In table 2, table 1 is shown with shade The region of "○".
[table 2]
As shown in Table 2, when the equivalent circle diameter φ of flat-bottom hole is 0.2mm and 0.25mm, if φ/d is 0.08 or more and small In 0.40, then flat-bottom hole can be detected.The equivalent circle diameter φ of flat-bottom hole be 0.3mm when, if φ/d be 0.1 less than 0.60, then it can detect flat-bottom hole.The equivalent circle diameter φ of flat-bottom hole be 0.4mm when, if φ/d be 0.11 less than 1.60, then it can detect flat-bottom hole.It should be noted that in JP2010-145401 bulletins, by actual measurement, φ/d is 0.06, it can not detect flat-bottom hole.Therefore, it was that the directly alignment of the focus of the ultrasonic wave emitted by ultrasound inspection head is flat in the past Bottom outlet.
(manufacturing method about simulated defect sample)
100mm × 100mm is cut out from the plate (raw material identical with the target of ultrasonic examination is carried out) of Al-0.5%Cu, so Afterwards using milling machine to as the ultrasonic wave plane of incidence face (surface) and its opposing face (back side) carry out facing cut respectively, be adjusted to 100mm×100mm×t20mm.Drill bit processing is carried out using gate machining center, the countersunk head of φ 9mm, depth 8mm are overleaf set Hole, then in the deep 2.0mm of the central portion of the bottom surface of counter sink setting φ 0.2mm (for the depth started from counter sink, from the back side The depth of start of calculation be 10mm) flat-bottom hole.
(method about the condition for using simulated defect sample adjustment ultrasonic examination measurement)
As measurement device, use " FSLINE " of Hitachi Power Solutions.It is being loaded with tap water In sink, simulated defect sample is set in such a way that surface becomes upper surface, the ultrasound inspection head of measurement device will be installed on " I3-1506S-50mm " (frequency 15MHz, focal length 50mm) is configured at the position of the surface 100mm of simulated defect sample. At this point, simulated defect sample, ultrasound inspection head are present in water.Then, to the upper surface of simulated defect sample (the 2nd face) Whole face carries out C-scan, confirms the position of counter sink.Ultrasound inspection head is moved to the surface of the counter sink confirmed, it will Ultrasound inspection head is configured at the position of surface 10mm of simulated defect sample or so, and confirm counter sink is reflected back wave height Degree.In the state of emitting ultrasonic wave by ultrasound inspection head, the ultrasonic wave waveform on computer picture is confirmed, detect surface reflection Echo, backside reflection echo and the reflection echo positioned at the counter sink between them.In order to set the reflection on thickness direction The detection zone of wave echo is provided with detection door in a manner of the reflection echo including surface reflection echo and counter sink (gate).It after the reflection echo for confirming counter sink, is operated and ultrasound inspection head is made periodically to be moved upward, visited The position for surveying ultrasound inspection head when being reflected back wave number maximum of counter sink is reflected back wave number maximum in counter sink, will The height of ultrasound inspection head is fixed, it is thus identified that focus is directed at the bottom surface of counter sink.At this point, in order to be observed in ultrasonic wave waveform To the reflection echo of flat-bottom hole, the position adjustment along the directions XY is also embodied.
After confirming the reflection echo for observing flat-bottom hole, is operated and ultrasound inspection head is made to be moved upward only 2.0mm (it is suitable with the depth to bottom surface of flat-bottom hole).Ultrasonic examination when being reflected back wave number maximum of detection flat-bottom hole The position of head, is reflected back wave number maximum in flat-bottom hole, the height of ultrasound inspection head is fixed, it is thus identified that focus alignment is flat The bottom surface of bottom outlet.Thus the state of the bottom surface of focus alignment flat-bottom hole is essentially become, is 0.1mm, gain measuring spacing therefore To carry out C-scan to simulated defect sample under conditions of 22dB, become with the detection range of the reflection echo of the bottom surface of flat-bottom hole Size is the area 0.03mm of the flat-bottom hole of φ 0.2mm2Mode, using the reflection echo intensity of the flat-bottom hole of φ 0.2mm as base It is accurate and the threshold value of defect level is set as 96 (can be used as when with the intensity of reflection echo being 96 or more defect be detected, The mode that the defect of φ 0.2mm can be used as the defect of φ 0.2mm and be detected is set).Then, will make detection door with Determination condition is stored in computer obtained from the thickness range to be measured (thickness for the target raw material to be measured) is adapted.
(inspection method about target raw material)
In such a way that thickness direction is parallel with the direction of illumination of ultrasonic wave, by the size φ 460mm dug out from milled sheet × The Al-0.5%Cu target raw material of t20mm configure in the sink for being loaded with tap water.Reading passes through method of adjustment system above-mentioned Fixed determination condition, the entire upper surface that the range (directions XY) that ultrasound inspection head scans will be made to be appointed as target, proceeds by Ultrasonic examination inspection.The result measured is compared with the threshold value of the defect level set by method of adjustment above-mentioned, It confirmed that the defect level of φ 0.2mm is not detected.
(manufacturing method about sputtering target)
Using NC lathes, to being that qualified target raw material are processed through ultrasonic examination inspection, then using based on heat The diffusion of platen press engages, and is engaged in the backer board of A2024 alloys.It after engagement, is finished, is molded using NC lathes For the sputtering target of the size of φ 450mm × t18.5mm.
Reference sign
1 ultrasound inspection head
2 inspected bodys
2a defects
5 sputtering targets
6 target raw material
7 supporting members
10,10A simulated defects sample
11 substrates
The 1st faces 11a
The 2nd faces 11b
12 counter sinks
The bottom surfaces 12a
13 flat-bottom holes
The bottom surfaces 13a
The 1st depth of d1
The 2nd depth of d2
The diameter (equivalent circle diameter) of 1 counter sinks of φ
The diameter (equivalent circle diameter) of 2 flat-bottom holes of φ

Claims (13)

1. simulated defect sample, the condition for being used for the ultrasonic examination measurement of the internal flaw to checking target raw material is adjusted It is whole,
The simulated defect sample has the substrate comprising the 1st face and 2nd face opposite with the 1st face,
It is formed with the counter sink with the 1st depth from the 1st surface side on the substrate, also, in the counter sink A part for bottom surface is formed with the flat-bottom hole with the 2nd depth from the bottom surface of the counter sink,
When the equivalent circle diameter φ of the flat-bottom hole is less than 0.3mm, the equivalent circle diameter φ of the flat-bottom hole is relative to described flat Ratio φ/d of 2nd depth d of bottom outlet is 0.08 less than 0.40,
The equivalent circle diameter φ of the flat-bottom hole be 0.3mm less than 0.4mm when, the equivalent circle diameter φ of the flat-bottom hole Ratio φ/d of the 2nd depth d relative to the flat-bottom hole is 0.1 less than 0.60,
When the equivalent circle diameter φ of the flat-bottom hole is 0.4mm or more, the equivalent circle diameter φ of the flat-bottom hole is relative to described Ratio φ/d of 2nd depth d of flat-bottom hole is 0.11 less than 1.60.
2. simulated defect sample as described in claim 1, wherein the equivalent circle diameter φ of the flat-bottom hole is 0.5mm or less.
3. simulated defect sample as claimed in claim 2, wherein the equivalent circle diameter φ of the flat-bottom hole is 0.1mm or more And it is less than 0.3mm.
4. simulated defect sample as described in claim 1, wherein the counter sink and the flat-bottom hole have multigroup.
5. simulated defect sample as described in any one of claims 1 to 4, wherein the substrate by aluminium, copper, titanium, silver or Including the alloy of at least one of these metallic elements is formed.
6. simulated defect sample as described in claim 1, wherein the condition that ultrasonic examination measures is for being with frequency The condition that the ultrasonic examination that the ultrasonic wave of 5MHz or more is implemented measures.
7. the manufacturing method of simulated defect sample, the simulated defect sample is used for the super of the internal flaw to checking target raw material The condition that sonic flaw detection measures is adjusted, and the manufacturing method has following processes：
It is formed from the 1st surface side with the 1st depth on the substrate comprising the 1st face and 2nd face opposite with the 1st face Counter sink process；With
A part in the bottom surface of the counter sink forms the flat-bottom hole with the 2nd depth from the bottom surface, the flat-bottom hole Equivalent circle diameter φ be less than 0.3mm when, make the equivalent circle diameter φ of the flat-bottom hole relative to the 2nd depth of the flat-bottom hole Ratio φ/d of d is 0.08 less than 0.40, the equivalent circle diameter φ of the flat-bottom hole be 0.3mm less than When 0.4mm, make the equivalent circle diameter φ of the flat-bottom hole relative to ratio φ/d of the 2nd depth d of the flat-bottom hole be 0.1 with Above and less than 0.60, when the equivalent circle diameter φ of the flat-bottom hole is 0.4mm or more, make the equivalent circle diameter φ of the flat-bottom hole Ratio φ/d of the 2nd depth d relative to the flat-bottom hole be 0.11 less than 1.60 process.
8. the manufacturing method of simulated defect sample as claimed in claim 7, wherein the substrate is by aluminium, copper, titanium, silver or packet Alloy containing at least one of these metallic elements is formed.
9. the method for adjustment of conditions of ultrasonic inspection, the method for adjustment has following processes：
By ultrasound inspection head, the 2nd from the substrate of simulated defect sample described in claim 1 is ultrasonic towards the 1st surface launching Wave, the process that the reflection echo of the counter sink of the simulated defect sample is confirmed；
Based on the reflection echo of the counter sink, the process for making the focus of the ultrasonic wave be directed at the bottom surface of the counter sink；
It receives by the reflection echo of the bottom reflection of the counter sink, and receives by the flat-bottom hole of the simulated defect sample The process of the reflection echo of bottom reflection；With
Based on the reflection echo from the flat-bottom hole, the focus of the ultrasonic wave is made to be directed at the work of the bottom surface of the flat-bottom hole Sequence.
10. method of adjustment as claimed in claim 9, wherein the condition that ultrasonic examination measures is for being 5MHz with frequency The condition that the ultrasonic examination that above ultrasonic wave is implemented measures.
11. the inspection method of target raw material, the inspection method has following processes：
Under conditions of the ultrasonic examination adjusted using the method for adjustment described in claim 9 or 10 is measured, on one side Ultrasound inspection head is set to be scanned the process for emitting ultrasonic wave to target raw material on one side；
The process for measuring the reflection echo reflected by the target raw material；With
Based on through it is described measure obtain as a result, the process of the internal flaw to judge the target raw material.
12. the manufacturing method of sputtering target, the manufacturing method has following processes：
Using the inspection method described in claim 11, come judge the target raw material internal flaw process；With
Implement the process of mechanical processing to being judged as the internal target raw material essentially without defect.
13. the manufacturing method of sputtering target, the manufacturing method has following processes：
Using the inspection method described in claim 11, come judge the target raw material internal flaw process；With
The process that will be judged as the internal target raw material essentially without defect and be engaged in supporting member.
CN201880000346.8A 2017-01-24 2018-01-18 Simulated defect sample and its manufacturing method, the method for adjustment of ultrasonic examination determination condition, the manufacturing method of the inspection method of target raw material and sputtering target Active CN108603862B (en)

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